EP2008978B1 - Procédé de fabrication d'une préforme pour fibres optiques à l'aide d'un procédé de dépôt de vapeur - Google Patents
Procédé de fabrication d'une préforme pour fibres optiques à l'aide d'un procédé de dépôt de vapeur Download PDFInfo
- Publication number
- EP2008978B1 EP2008978B1 EP08011104A EP08011104A EP2008978B1 EP 2008978 B1 EP2008978 B1 EP 2008978B1 EP 08011104 A EP08011104 A EP 08011104A EP 08011104 A EP08011104 A EP 08011104A EP 2008978 B1 EP2008978 B1 EP 2008978B1
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- EP
- European Patent Office
- Prior art keywords
- substrate tube
- deposition
- hollow substrate
- tube
- intermediate step
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000005137 deposition process Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 230000003287 optical effect Effects 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 92
- 230000008021 deposition Effects 0.000 claims abstract description 40
- 238000005530 etching Methods 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 29
- 239000011521 glass Substances 0.000 claims description 19
- 239000010453 quartz Substances 0.000 claims description 16
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 claims description 8
- 238000007496 glass forming Methods 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 claims description 2
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004071 soot Substances 0.000 description 19
- 239000000377 silicon dioxide Substances 0.000 description 10
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- 229910003910 SiCl4 Inorganic materials 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 4
- 229910006113 GeCl4 Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 150000002222 fluorine compounds Chemical class 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910006111 GeCl2 Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- BWTZYYGAOGUPFQ-UHFFFAOYSA-N difluoroacetylene Chemical compound FC#CF BWTZYYGAOGUPFQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- QHGIKMVOLGCZIP-UHFFFAOYSA-N germanium dichloride Chemical compound Cl[Ge]Cl QHGIKMVOLGCZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01815—Reactant deposition burners or deposition heating means
- C03B37/01823—Plasma deposition burners or heating means
- C03B37/0183—Plasma deposition burners or heating means for plasma within a tube substrate
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01815—Reactant deposition burners or deposition heating means
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
- C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/31—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with germanium
Definitions
- the present invention relates to a method for manufacturing a preform for optical fibres by means of a vapour deposition process, which method comprises the steps of:
- the cylindrical inner surface of an elongated, vitreous substrate tube (for example made of quartz) is coated with layers of doped or undoped silica (for example germanium-doped silica).
- doped or undoped silica for example germanium-doped silica.
- silica as used herein is to be understood to mean any substance in the form of SiO x , whether or not stoichiometric, and whether or not crystalline or amorphous. This can be effected by positioning the substrate tube along the cylindrical axis of the resonance cavity, and flushing the interior of the tube with a gaseous mixture comprising O 2 , SiSl 4 and GeCl 2 (for example).
- a localised plasma is concurrently generated within the cavity, causing the reaction of Si, O and Ge so as to thus effect direct deposition of, for example, Ge-doped SiO x on the inner surface of the substrate tube. Since such deposition only occurs in the vicinity of the localised plasma, the resonant cavity (and thus the plasma) must be swept along the cylindrical axis of the tube in order to uniformly coat the tube along the entire length thereof.
- the tube is thermally collapsed into a massive rod having a Ge-doped silica core portion and a surrounding undoped silica cladding portion.
- a thin glass fibre can be drawn from the rod and be wound on a reel; said fibre then has a core portion and a cladding portion corresponding to those of the rod.
- the Ge-doped core has a higher refractive index than the undoped cladding, the fibre can function as a waveguide, for example for use in propagating optical telecommunication signals.
- the gaseous mixture flushed through the substrate tube may also contain other components; the addition of C 2 F 6 , for example, leads to a reduction in the refractive index value of the doped silica.
- the preform rod may be externally coated with an additional glass layer, for example by applying silica by means of a deposition process, or by placing the preform rod in a so-called jacket tube (comprised of undoped silica) prior to the drawing procedure, so as to thus increase the amount of undoped silica relative to the amount of doped silica in the final fibre.
- optical fibre for telecommunication purposes requires that the optical fibre be substantially free from defects (for example discrepancies in the percentage of dopants, undesirable cross-sectional ellipticity and the like), because, when considered over a large length of the optical fibre, such defects may cause a significant attenuation of the signal being transported. It is important, therefore, to realise a very uniform and reproducible PCVD process, because the quality of the deposited PCVD layers will eventually determine the quality of the fibres.
- defects for example discrepancies in the percentage of dopants, undesirable cross-sectional ellipticity and the like
- U.S. 4,493,721 relates to a method of manufacturing an optical fiber comprising the steps of:
- U.S. 2006/0230793 A1 relates to a method for manufacturing an optical fiber preform by MCVD comprising: an etching/collapsing process for etching and collapsing a quartz tube at the same time by injecting an reaction gas for etching into the quartz tube together with heating the tube at a higher temperature than a softening temperature so that the inner diameter of the tube is optimized just before a following closing process.
- a device for manufacturing a preform for optical fibres by means of a vapour deposition process is known per se from Korean patent application No. 2003-774,952 .
- an optical preform is made by means of an MCVD (Modified Chemical Vapour Deposition) process, in which a discharge tube and an insert tube are used, which discharge tube is attached to the substrate tube.
- the insert tube is disposed within the discharge tube and has an external diameter which is smaller than that of the discharge tube.
- a soot scraping element Disposed within the insert tube is a soot scraping element, which comprises a bar which rotates in the interior of the insert tube and which is in contact with the inner surface thereof.
- an annular space Between the insert tube and the discharge tube is an annular space, through which gases are passed.
- a device for manufacturing an optical preform by means of an internal vapour deposition process wherein a tubular element is mounted at the pump side of a substrate for the removal of solid, undeposited particles.
- a device comprises a screw structure which follows the inner surface of the tubular element, which screw structure comprises an open gas conduit which is spiral-shaped and rotatable.
- low-quality quartz layers may be deposited, in particular in the area outside the range of movement of the energy source being reciprocated along the length of the substrate tube, viz. the resonator.
- soot rings so-called soot rings, but also but also quartz having a high internal stress caused by a high dopant content.
- the present inventors have found that such low quality quartz present in the interior of the substrate tube may adversely affect the substrate tube, in particular as a result of the formation of gas bubbles in the vicinity of the supply side of the substrate tube upon collapsing the hollow substrate tube into a solid preform.
- the present inventors have found that such low quality quartz may come loose from the interior of the hollow substrate tube during the collapsing process, which may lead to contamination or to the formation of gas bubbles elsewhere in the substrate tube.
- Another negative aspect is the fact that cracks may occur in the low quality quartz region, which cracks may propagate in the direction of the centre of the substrate tube, which is undesirable.
- the present inventors have furthermore found that the low quality quartz may lead to clogging of the substrate tube and the associated piping, as a result of which the pressure may increase to an undesirably high value during the deposition process, which will have an adverse effect the deposition process in the substrate tube, which effect will be perceived as a white colour in practice.
- the substrate tube itself is made of high-quality quartz. In practice, however, the total length of the substrate tube will be greater than the length of the part of the substrate tube that is eventually converted into a glass fibre by means of a drawing process, because the two ends of the substrate tube, where deposition takes place, may cause undesirable side effects, viz. deposition defects, contamination, formation of bubbles and the like.
- the present inventors have in particular found that, in the situation in which a so-called insert tube is used on the discharge side of the hollow substrate tube, the deposition of soot in particular occurs at high deposition rates, notably deposition processes in which the deposition of glass layers takes place at a rate of more than 3 g/minute, which processes generally last longer than 5 hours.
- Such an insert tube has an external diameter which is smaller than the internal diameter of the hollow substrate tube itself, and generally it is disposed within the substrate tube with a close fit, near the discharge side thereof.
- the pressure within the hollow substrate tube will increase, so that the deposition efficiency of SiCl 4 will decrease further and (even) more soot will be formed, which is undesirable.
- Such a process is self-reinforcing, which means that the deposition process will have to be terminated due to a complete blockage of the passage of the insert tube on the discharge side of the hollow substrate tube. The interruption of the deposition process is to be considered undesirable.
- the object of the present invention is thus to provide a method for manufacturing a preform for optical fibres in which the risk of clogging of the insert tube near the discharge side of the hollow substrate tube is minimised.
- Another object of the present invention is to provide a method for manufacturing a preform for optical fibres in which the deposition process does not have to be terminated unnecessarily due to clogging in spite of the fact that high deposition rates and long process times are used.
- the present invention as referred to in the introduction is characterised in that the deposition of glass layers on the inner surface of the hollow substrate tube is interrupted during step iii) by carrying out at least one intermediate step, which intermediate step comprises the supplying of an etching gas to the supply side of the hollow substrate tube, whilst the supply of the doped or undoped glass-forming gases is stopped during the intermediate step, and the possible continuation of the deposition process after termination of the intermediate step.
- the present inventors have found that the initial position and the exact distribution of the deposition of glass layers on the interior of the hollow substrate tube depends on a number of process conditions, such as the plasma power that is used, the pressure inside the hollow substrate tube, the configuration of the resonator and the deposition rate.
- the present inventors have thus found that a small fraction of the glass layers is deposited on the interior of the insert tube near the discharge side of the hollow substrate tube during the PCVD process.
- a certain amount of soot is deposited at that location instead of quartz.
- the thus deposited material viz.
- soot has a much higher specific volume than quartz, so that even a small amount of soot may lead to clogging of the insert tube.
- soot material may come loose from the interior of the hollow substrate tube and lead to contaminations elsewhere in the substrate tube.
- a deposition phase comprises the supplying of glass-forming components in a carrier gas, such as SiCl 4 , GeCl 4 , C 2 F 2 and O 2 , on the supply side of the hollow substrate tube.
- the intermediate step only a halogen-containing gas is supplied to the interior of the hollow substrate tube via the supply side thereof, which etching gas may be provided with a carrier gas or flushing gas, such as oxygen.
- the intermediate step is in fact terminated by resuming the supply of the glass-forming gases to the interior of the hollow substrate tube, possibly in combination with dopants that change (increase, decrease) the refractive index.
- dopants that change (increase, decrease) the refractive index.
- step index preform it is possible to carry out the intermediate step within a deposition phase itself, whilst for a so-called gradient index preform an interruption within a deposition phase itself is considered to be disadvantageous, because it leads to an undesirable profile disturbance.
- intermediate step according to the present invention between one deposition phase and the next deposition phase(s), which deposition phases may lead to different glass compositions, possibly resulting in different refractive index values.
- the soot present in the insert tube is effectively etched away when such an intermediate step is used, so that any clogging of the insert tube is prevented.
- the deposition of glass layers is resumed. It is preferable, therefore, to carry out the aforesaid intermediate step each time between two deposition phases.
- the etching gas used in the present invention is preferably a halogen-containing gas, in particular of fluorine-containing gas, in particular selected from the group consisting of CCl 2 F 2 , CF 4 , C 2 F 6 , SF 6 , F 2 and SO 2 F 2 , or a combination thereof, in which case the fluorine-containing gas may be present in a flushing gas.
- fluorine-containing gas in particular selected from the group consisting of CCl 2 F 2 , CF 4 , C 2 F 6 , SF 6 , F 2 and SO 2 F 2 , or a combination thereof, in which case the fluorine-containing gas may be present in a flushing gas.
- C 2 F 6 and SF 6 are preferred etching gases.
- the intermediate step is preferably carried out for a period of 5 - 15 minutes, whilst it is in particular preferable if the substrate tube is rotated during said intermediate step.
- the plasma moves back and forth along the longitudinal axis of the hollow substrate tube, between the point of reversal near the supply side and the point of reversal near the discharge side of the hollow substrate tube, during step iii), it is possible in a special embodiment for the plasma to be present near the point of reversal near the discharge side of the hollow substrate tube during the intermediate step.
- the intermediate step is in particular carried out at a position where the deposition of soot is predominant, viz. near the discharge side of the hollow substrate tube, in particular in the insert tube that is disposed on the aforesaid side.
- the plasma power that is used may be set to a value of maximally 10 kW, in particular to a value of maximally 5 kW, so that in particular melting of the substrate tube and/or the insert tube is prevented.
- the present invention is in particular suitable for manufacturing preforms from which single-mode optical fibres are obtained, but the present invention may also be suitably used for removing layers having a high germanium content from the entire interior of the preform after termination of step iii), which layers are responsible for the occurrence of layer cracking when the hollow substrate tube is subjected to a consolidation treatment for manufacturing the solid preform. The risk of layer cracking is prevented by thus removing layers having a high germanium content.
- the present invention will be explained hereinafter by means of an example, in which connection it should be noted, however, that the present invention is by no means limited to such special examples.
- the figure is a schematic representation of the equipment used in the deposition process.
- a hollow substrate tube 2 made of quartz was manufactured by means of a standard PCVD process as known from Dutch patent NL 1 023 438 in the name of the present applicant.
- the hollow substrate tube 2 having a supply side 5 and a discharge side 6 was placed in a furnace 1, in which furnace 1 a resonator 3 is present, which resonator 3 can move back and forth along the length of the hollow substrate tube 2 within the furnace 1.
- Microwave energy was supplied to the resonator 3 via the waveguide 4 so as to create plasma conditions in the interior 7 of the hollow substrate tube 2, which plasma conditions function to deposit glass layers on the interior 7 of the hollow substrate tube 2.
- insert tube Disposed within the hollow substrate tube 2, near the discharge side 6 of the hollow substrate tube 2, is a so-called insert tube (not shown), in which insert tube deposition of soot takes place near the location indicated at 9.
- Such an insert tube has an external diameter which is smaller than the internal diameter of the hollow substrate tube 2 itself, and generally it is disposed within the substrate tube 2 with a close fit, near the discharge side 6 thereof.
- the present inventors have found that the plasma generated by the resonator 3 may be present slightly outside the resonator 3, in which case the plasma in particular exits the resonator 3 in the vicinity of the discharge side 6, near the insert tube.
- soot As a result of the aforesaid deposition of soot, the effective cross-sectional area in the insert tube was reduced, resulting in a pressure increase inside the hollow substrate tube 2, which adversely affected the deposition process.
- soot rings were visually perceptible during the deposition process.
- the present application is in particular aimed at removing such soot deposition at any desired moment, in particular during the deposition process.
- An internal chemical vapour deposition process was carried out by moving the plasma back and forth along the length of a hollow substrate tube 2 at a velocity of 20 m/min, which hollow substrate tube 2 was positioned in the interior of a furnace 1.
- the furnace 1 was set to a temperature of 1000 °C, using a plasma power of 9 kW.
- the deposition rate of glass layers on the interior of the thus positioned hollow substrate tube 2 was 3.1 g/min, based on SiO 2 , with the pressure inside the hollow substrate tube 2 amounting to about 10 mbar.
- a gas composition consisting of O 2 , SiCl 4 , GeCl 4 and C 2 F 6 was supplied to the interior 7 of the hollow substrate tube 2.
- the deposition of glass layers on the interior 7 of the hollow substrate tube 2 was interrupted and subsequently the resonator 3, in particular the element in which a plasma is generated, was moved in the direction of the discharge side 6 of the hollow substrate tube 2.
- a distinct contamination with soot was perceptible in the interior of the hollow substrate tube 2, near the discharge side 6 of which an insert tube is disposed.
- the intermediate step according to the present invention was carried out, during which intermediate step the temperature of the furnace was maintained at 1000 °C. The plasma power was reduced to 5 kW.
- the composition of the gases supplied to the interior 7 of the hollow substrate tube 2 was changed into an etching gas composition consisting of a fluorine-containing compound and oxygen, in particular with a delivery rate of 3 standard litres of O 2 per minute and 0.3 standard litres of C 2 F 6 per minute.
- the intermediate step was carried out for 5-10 minutes, during which the hollow substrate tube 2 was continuously rotated. After termination of the intermediate step thus carried out it was established that hardly any soot was left in the insert tube in the vicinity of the discharge side 6. After soot had been removed in the above-described manner, the deposition process was resumed, in particular by supplying a gas composition consisting of O 2 , SiCl 4 , GeCl 4 and C 2 F 6 to the interior of the hollow substrate tube 2.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Plasma & Fusion (AREA)
- Physics & Mathematics (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Surface Treatment Of Glass (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
Claims (10)
- Procédé de fabrication d'une préforme pour des fibres optiques par le biais d'un processus de dépôt en phase vapeur, lequel procédé comprend les étapes consistant à :i) prévoir un tube substrat en quartz verre (2) creux ayant un côté d'alimentation (5) et un côté de décharge (6)ii) alimenter en gaz de formation de verre dopés ou non dopés l'intérieur du tube substrat (2) creux depuis son côté d'alimentation (5)iii) créer des conditions de température et de plasma à l'intérieur du tube substrat (2) creux pour déposer des couches de verre sur la surface interne du tube substrat (2) creux, lequel dépôt peut être considéré comme comprenant un nombre de phases séparées, chaque phase ayant une valeur d'indice de réfraction initiale et une valeur d'indice de réfraction finale et comprenant le dépôt d'un nombre de couches de verre à l'intérieur (7) du tube substrat (2) creux durant une certaine période de temps, le plasma étant déplacé en va-et-vient le long de l'axe longitudinal du tube substrat (2) creux entre un point d'inversion proche du côté d'alimentation (5) et un point d'inversion proche du côté de décharge (6) du tube substrat (2) creux, et éventuellementiv) consolider le tube substrat (2) obtenu après l'étape iii) dans la préforme, caractérisé en ce que le dépôt de couches de verre sur la surface interne du tube substrat (2) creux est interrompu pendant l'étape iii) en exécutant au moins une étape intermédiaire, laque étape intermédiaire comprend le fait d'alimenter le côté d'alimentation (5) du tube substrat (2) creux en un gaz de gravure, tandis que l'alimentation en gaz de formation de verre dopés ou non dopés est arrêtée durant l'étape intermédiaire, et la poursuite éventuelle du processus de dépôt après l'achèvement de l'étape intermédiaire.
- Procédé selon la revendication 1, caractérisé en ce qu'un gaz de gravure contenant du fluor est utilisé.
- Procédé selon l'une quelconque ou plusieurs des revendications précédentes, caractérisé en ce que le gaz de gravure est choisi dans le groupe constitué de CCl2F2, de CF4, de C2F6, de SF6, de F2 et de SO2F2, ou leur combinaison, éventuellement en la présence d'un gaz de rinçage, tel que de l'oxygène.
- Procédé selon la revendication 3, caractérisé en ce que le gaz de gravure est une combinaison de C2F6 et de O2.
- Procédé selon l'une quelconque ou plusieurs des revendications précédentes, caractérisé en ce que l'étape intermédiaire est exécutée pendant une période de 5 à 15 minutes.
- Procédé selon l'une quelconque ou plusieurs des revendications précédentes, caractérisé en ce que le tube substrat est en rotation durant ladite étape intermédiaire.
- Procédé selon l'une quelconque ou plusieurs des revendications précédentes, caractérisé en ce que le plasma est présent à proximité du point d'inversion proche du côté de décharge du tube substrat creux durant l'étape intermédiaire.
- Procédé selon la revendication 7, caractérisé en ce que la puissance du plasma est réglée à une valeur de 10 kW au maximum.
- Procédé selon la revendication 8, caractérisé en ce que la puissance du plasma est réglée à une valeur de 5 kW au maximum.
- Procédé selon l'une quelconque ou plusieurs des revendications précédentes, caractérisé en ce que l'étape intermédiaire est exécutée entre une phase de dépôt et la/les phase(s) de dépôt suivante(s) à l'étape iii).
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL1034059A NL1034059C2 (nl) | 2007-06-29 | 2007-06-29 | Werkwijze voor het vervaardigen van een voorvorm voor optische vezels onder toepassing van een dampdepositieproces. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP2008978A1 EP2008978A1 (fr) | 2008-12-31 |
| EP2008978B1 true EP2008978B1 (fr) | 2010-09-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP08011104A Not-in-force EP2008978B1 (fr) | 2007-06-29 | 2008-06-19 | Procédé de fabrication d'une préforme pour fibres optiques à l'aide d'un procédé de dépôt de vapeur |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US8168267B2 (fr) |
| EP (1) | EP2008978B1 (fr) |
| JP (1) | JP5490379B2 (fr) |
| CN (1) | CN101333067B (fr) |
| AT (1) | ATE481365T1 (fr) |
| BR (1) | BRPI0802237B1 (fr) |
| DE (1) | DE602008002481D1 (fr) |
| NL (1) | NL1034059C2 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9643879B2 (en) | 2013-07-01 | 2017-05-09 | Draka Comteq B.V. | Method for manufacturing a precursor for a primary preform for optical fibres by a plasma deposition process |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8741394B2 (en) * | 2010-03-25 | 2014-06-03 | Novellus Systems, Inc. | In-situ deposition of film stacks |
| NL2004544C2 (nl) | 2010-04-13 | 2011-10-17 | Draka Comteq Bv | Inwendig dampdepositieproces. |
| NL2004546C2 (nl) * | 2010-04-13 | 2011-10-17 | Draka Comteq Bv | Inwendig dampdepositieproces. |
| NL2006962C2 (nl) | 2011-06-17 | 2012-12-18 | Draka Comteq Bv | Inrichting en werkwijze voor het vervaardigen van een optische voorvorm. |
| NL2007831C2 (en) * | 2011-11-21 | 2013-05-23 | Draka Comteq Bv | Apparatus and method for carrying out a pcvd deposition process. |
| NL2009962C2 (en) * | 2012-12-11 | 2014-06-12 | Draka Comteq Bv | Method for activating an inner surface of a hollow glass substrate tube for the manufacturing of an optical fiber preform. |
| US9002162B2 (en) * | 2013-03-15 | 2015-04-07 | Ofs Fitel, Llc | Large core multimode optical fibers |
| NL2010724C2 (en) | 2013-04-26 | 2014-10-29 | Draka Comteq Bv | A pcvd method for manufacturing a primary preform for optical fibers. |
| NL2012857B1 (en) * | 2014-05-22 | 2016-03-07 | Draka Comteq Bv | Apparatus and method for carrying out a plasma deposition process. |
| NL2015162B1 (en) * | 2015-07-13 | 2017-02-01 | Draka Comteq Bv | Method for activating an inner surface of a substrate tube for the manufacturing of an optical fiber preform. |
| NL2015161B1 (en) * | 2015-07-13 | 2017-02-01 | Draka Comteq Bv | A method for preparing a primary preform by etching and collapsing a deposited tube. |
| NL1041529B1 (en) * | 2015-10-16 | 2017-05-02 | Draka Comteq Bv | A method for etching a primary preform and the etched primary preform thus obtained. |
| DE102018132338B3 (de) * | 2018-12-14 | 2019-11-21 | Leibniz-Institut für Photonische Technologien e. V. | Partikelfreies verfahren zur signifikanten reduzierung der oberflächenrauhigkeit von rohren, kapillaren und hohlfasern aus kieselglas oder hoch kieselhaltigen gläsern und optischen gläsern sowie zur reinigung von kavitätenoberflächen von rohren, kapillaren und hohlfasen aus kieselglas oder hoch kieselglashaltigen optischen gläsern |
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| NL8201453A (nl) * | 1982-04-06 | 1983-11-01 | Philips Nv | Werkwijze voor de vervaardiging van optische vezels. |
| US4630890A (en) * | 1983-06-22 | 1986-12-23 | At&T Bell Laboratories | Exposed core optical fibers, and method of making same |
| FI78891C (fi) * | 1987-09-11 | 1989-10-10 | Nokia Oy Ab | Anordning foer avlaegsnande av pulverformigt material som samlas i den roerformiga bakdelen vid tillverkning av en optisk fibers aemne. |
| FI83944C (fi) | 1989-05-19 | 1991-09-25 | Rautaruukki Oy | Stoedben till en paohaengsvagn. |
| CN2284105Y (zh) * | 1996-11-08 | 1998-06-17 | 蒙里声 | 环状尖端脉冲等离子体除尘器 |
| US6105396A (en) * | 1998-07-14 | 2000-08-22 | Lucent Technologies Inc. | Method of making a large MCVD single mode fiber preform by varying internal pressure to control preform straightness |
| DE19852704A1 (de) * | 1998-11-16 | 2000-05-18 | Heraeus Quarzglas | Verfahren zur Herstellung einer Vorform für eine optische Faser und für die Durchführung des Verfahrens geeignetes Substratrohr |
| US6718800B2 (en) * | 1999-03-08 | 2004-04-13 | Fitel Usa Corp. | Method of collapsing a tube for an optical fiber preform |
| CN1277888A (zh) * | 2000-06-02 | 2000-12-27 | 黄立维 | 一种有机废气的净化方法 |
| CA2355819A1 (fr) * | 2000-08-28 | 2002-02-28 | Sumitomo Electric Industries, Ltd. | Fibre optique, methode de fabrication d'une preforme, et methode de fabrication de la fibre optique |
| JP3775234B2 (ja) * | 2001-03-29 | 2006-05-17 | 住友電気工業株式会社 | 光ファイバ母材の製造方法 |
| JP2003012338A (ja) * | 2001-06-29 | 2003-01-15 | Sumitomo Electric Ind Ltd | Mcvd法を用いた光ファイバ母材の製造方法 |
| WO2003052173A1 (fr) * | 2001-12-14 | 2003-06-26 | Corning Incorporated | Procede de gravure a deux etapes pour une preforme de fibres optiques |
| US7169440B2 (en) * | 2002-04-16 | 2007-01-30 | Tokyo Electron Limited | Method for removing photoresist and etch residues |
| US6988380B2 (en) * | 2002-08-15 | 2006-01-24 | Ceramoptec Industries, Inc. | Method of silica optical fiber preform production |
| WO2004023175A1 (fr) * | 2002-09-03 | 2004-03-18 | Lg Cable Ltd. | Procede de fabrication de preforme de fibre optique presentant au final une faible dispersion de polarisation de mode grace a l'amelioration d'ovalisation |
| US20060230793A1 (en) * | 2002-11-07 | 2006-10-19 | Choon-Keun Hong | Method for manufacturing an optical fiber preform by mcvd |
| US20040107734A1 (en) * | 2002-12-04 | 2004-06-10 | Paresh Kenkare | Systems and methods for fabricating optical fiber preforms |
| NL1023438C2 (nl) | 2003-05-15 | 2004-11-22 | Draka Fibre Technology Bv | Werkwijze ter vervaardiging van een optische vezel, voorvorm en een optische vezel. |
| NL1025155C2 (nl) * | 2003-12-30 | 2005-07-04 | Draka Fibre Technology Bv | Inrichting voor het uitvoeren van PCVD, alsmede werkwijze voor het vervaardigen van een voorvorm. |
| JP4552599B2 (ja) * | 2004-10-29 | 2010-09-29 | 住友電気工業株式会社 | 光ファイバ母材の製造方法 |
| KR100774952B1 (ko) | 2005-04-14 | 2007-11-09 | 엘지전자 주식회사 | 플라즈마 디스플레이 장치, 플라즈마 디스플레이 패널 및그의 제조방법 |
| JP2006248824A (ja) * | 2005-03-09 | 2006-09-21 | Sumitomo Electric Ind Ltd | ガラスの製造方法及びガラスの製造装置 |
| JP2007084362A (ja) * | 2005-09-20 | 2007-04-05 | Sumitomo Electric Ind Ltd | 光ファイバー母材の製造方法 |
| ATE512937T1 (de) * | 2005-10-27 | 2011-07-15 | Sterlite Technologies Ltd | Verfahren zur herstellung einer vorform für optische fasern |
| NL1030749C2 (nl) * | 2005-12-22 | 2007-06-25 | Draka Comteq Bv | Inrichting en werkwijze voor het vervaardigen van een optische voorvorm. |
| US8020410B2 (en) * | 2007-11-15 | 2011-09-20 | Corning Incorporated | Methods for making optical fiber preforms and microstructured optical fibers |
-
2007
- 2007-06-29 NL NL1034059A patent/NL1034059C2/nl not_active IP Right Cessation
-
2008
- 2008-06-19 AT AT08011104T patent/ATE481365T1/de not_active IP Right Cessation
- 2008-06-19 DE DE602008002481T patent/DE602008002481D1/de active Active
- 2008-06-19 EP EP08011104A patent/EP2008978B1/fr not_active Not-in-force
- 2008-06-25 JP JP2008165433A patent/JP5490379B2/ja not_active Expired - Fee Related
- 2008-06-27 BR BRPI0802237-2A patent/BRPI0802237B1/pt not_active IP Right Cessation
- 2008-06-27 US US12/147,535 patent/US8168267B2/en not_active Expired - Fee Related
- 2008-06-27 CN CN2008101273547A patent/CN101333067B/zh active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9643879B2 (en) | 2013-07-01 | 2017-05-09 | Draka Comteq B.V. | Method for manufacturing a precursor for a primary preform for optical fibres by a plasma deposition process |
Also Published As
| Publication number | Publication date |
|---|---|
| BRPI0802237A2 (pt) | 2009-02-25 |
| JP2009013053A (ja) | 2009-01-22 |
| ATE481365T1 (de) | 2010-10-15 |
| DE602008002481D1 (de) | 2010-10-28 |
| EP2008978A1 (fr) | 2008-12-31 |
| US20090004404A1 (en) | 2009-01-01 |
| JP5490379B2 (ja) | 2014-05-14 |
| CN101333067A (zh) | 2008-12-31 |
| US8168267B2 (en) | 2012-05-01 |
| BRPI0802237B1 (pt) | 2018-06-26 |
| CN101333067B (zh) | 2013-10-23 |
| NL1034059C2 (nl) | 2008-12-30 |
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